Analytical methods published in the last 20 years for the extraction, chromato-graphic separation, and quantification of alkylphenol ethoxylates (APEO) and related compounds in environmental samples are reviewed. Examples of various isolation and preconcentration techniques for water, effluent, sediment and sludge are presented. This includes procedures from the classical liquid-liquid and Soxhlet extraction to the up-to-date solid phase and supercritical fluid extraction. Chromatographic separation of APEO by normal and reversed phase liquid chromatography (LC) and capillary column gas chromatography (GC) is compared. A variety of quantification methods involving the common LC and GC detectors as well as various mass spectrometric techniques are also discussed.